반응 #595356

반응 방정식

compound

2-Amino-4-[4-(2-hydroxyethoxy)phenyl]-6-(phenylsulfanyl)pyridine-3,5-dicarbonitrile

sodium hydroxide

→

6-Amino-4-[4-(2-hydroxyethoxy)phenyl]-2-oxo-1,2-dihydropyridine-3,5-dicarbonitrile

용매

ethanol

반응 조건

후처리

1. 1
   기타a clear solution is formed
2. 2
   온도After cooling to RT
3. 3
   기타the solvent is removed on a rotary evaporator
4. 4
   기타is formed
5. 5
   workup.STIRRINGThe suspension is stirred at RT for 3 h
6. 6
   여과The precipitate is filtered off
7. 7
   세척washed with about 5 ml of water
8. 8
   기타a little ethanol and then recrystallized from about 10 ml of ethanol
9. 9
   기타The product obtained in this manner
10. 10
    기타is used without further purification in the subsequent reactions

실험 절차

500 mg (1.29 mmol) of the compound from Example 99A are initially charged in 6.4 ml of ethanol. After addition of 2.57 g (28.96 mmol) of sodium hydroxide, the mixture is stirred at 80° C. for 30 min, and a clear solution is formed. After cooling to RT, the solvent is removed on a rotary evaporator. The residue is taken up in 3 ml of water and acidified with 1 N hydrochloric acid until a yellowish precipitate is formed. The suspension is stirred at RT for 3 h. The precipitate is filtered off, washed with about 5 ml of water and a little ethanol and then recrystallized from about 10 ml of ethanol. The product obtained in this manner is used without further purification in the subsequent reactions.

출처